CN115207295A - Novel glassy state electrode material of lithium ion battery and preparation method thereof - Google Patents

Novel glassy state electrode material of lithium ion battery and preparation method thereof Download PDF

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CN115207295A
CN115207295A CN202110375525.3A CN202110375525A CN115207295A CN 115207295 A CN115207295 A CN 115207295A CN 202110375525 A CN202110375525 A CN 202110375525A CN 115207295 A CN115207295 A CN 115207295A
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electrode material
lithium ion
ion battery
source compound
lithium
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方学舟
郭艳艳
吕景文
刘经英
于猛
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Changchun University of Science and Technology
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C12/00—Powdered glass; Bead compositions
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/582—Halogenides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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Abstract

The invention relates to a novel glassy state electrode material of a lithium ion battery and a preparation method thereof. The invention uses compounds containing elements such as lithium, vanadium, iron, phosphorus and the like as raw materials to obtain the novel glassy state electrode material of the lithium ion battery by a melting quenching method. Compared with the traditional crystalline electrode material, the lithium ion is subjected to surface reaction on the material in the process of intercalation and deintercalation, so that the structural stress on the material is smaller, and the material has more stable electrochemical performance. The invention has wide source of raw materials, low price, simple process and easy large-scale production, and can be used as the electrode of the lithium ion battery.

Description

Novel glassy state electrode material of lithium ion battery and preparation method thereof
Technical Field
The invention belongs to the field of lithium ion battery anode materials, and relates to a novel lithium ion battery glassy state electrode material and a preparation method thereof.
Background
The secondary battery plays an important role in the field of electrochemical energy storage, wherein the lithium ion battery has the advantages of high electrochemical performance, no memory effect, environmental protection and the like, and is a main energy storage device in the fields of electronic equipment and electric automobiles. The specific energy of the battery mainly depends on the specific capacity and the potential difference of the anode material and the cathode material, and the high-energy battery requires the anode material to have high potential and the cathode material to have low potential. The structural stability of the electrode material has a great influence on the basic electrochemical performance of the battery, and generally, the performance (such as capacity and voltage) of the positive electrode material is considered to be a key factor determining the energy density, safety, cycle life and the like of the battery at present, the positive electrode material of the lithium ion battery mainly comprises lithium nickelate, olivine lithium iron phosphate, spinel lithium manganate and lithium cobaltate, but the traditional positive electrode material of the lithium ion battery is gradually eliminated due to a series of defects of difficult synthesis conditions, poor thermal stability, high price and the like, and therefore, the search for a novel positive electrode material with high capacity, high multiplying power and long cycle life has become a research hotspot in recent years.
Compared with the traditional crystalline state electrode material, the lithium ions are de-intercalated in the glassy state anode material and react on the surface of the material, so that the structural stress of the material is small, the distortion degree of the material is low, and the material has stable electrochemical performance. The invention has wide raw material source, low price, simple process and easy large-scale production, and can be used for assembling the lithium ion battery.
Disclosure of Invention
The invention provides a novel glassy state electrode material of a lithium ion battery and a preparation method thereof. By component design, the glassy state electrode material with stable chemical performance, good thermal stability, higher specific capacity and better cycle performance is obtained.
The technical scheme is as follows:
the invention relates to a novel glassy state electrode material of a lithium ion battery and a preparation method thereof, wherein the preparation method comprises the following steps:
1) Designing the components according to a formula, accurately weighing a lithium source compound, a vanadium source compound, an iron source compound, a phosphate source compound and a fluorine source compound, and grinding in a mortar to uniformly mix the materials;
2) Putting the uniformly mixed raw materials into a corundum crucible, placing the corundum crucible into a silicon-carbon rod resistance furnace, and melting at high temperature to obtain molten and clarified glass liquid;
3) Pouring the obtained molten clear glass liquid on a mold, transferring the molten clear glass liquid to a template at room temperature after the glass is solidified, and naturally cooling the glass;
4) And (3) placing the prepared glass material in an agate mortar, grinding the glass material into fine particles, grinding the fine particles by a wet method to obtain glass powder with moderate particle size, and drying to obtain the glassy state electrode material of the lithium ion battery.
Wherein:
the lithium source compound in the step 1) is one or more of lithium carbonate, lithium hydroxide and lithium fluoride;
the vanadium source compound in the step 1) is one or more of vanadium pentoxide, ammonium metavanadate, vanadium hydroxide and vanadium tetrafluoride;
the iron source compound in the step 1) is one or more of ferric oxide, ferric hydroxide and ferric fluoride;
the phosphorus source compound in the step 1) is one or more of phosphorus pentoxide, ammonium dihydrogen phosphate and ammonium monohydrogen phosphate;
the fluorine source compound in the step 1) is one or more of lithium fluoride, ferric fluoride, hydrofluoric acid, vanadium tetrafluoride and ammonium fluoride.
In the step 3), the melting temperature is 1200-1300 ℃, and the melting time is 30-45 min;
in the step 4), the temperature of the die is 250-300 ℃;
in the step 5), the wet grinding refers to adding absolute ethyl alcohol, and the grinding time is 3-4 h.
The invention has the technical effects that the physicochemical property and the electrochemical property of the material achieve the win-win effect through component design. In addition, the glassy electrode material reacts on the surface of the material in the lithium ion extraction process, so that the structural stress generated on the material is small, and the material has low distortion degree, so that the material has better cycle stability. The invention has wide source of raw materials, low price, simple process, easy large-scale production and contribution to realizing commercial application.
Drawings
FIG. 1 is an XRD pattern of sample # 1 in accordance with an exemplary embodiment;
FIG. 2 is a constant current charge and discharge curve of sample # 1 in accordance with an exemplary embodiment;
figure 3 is a cycle performance curve of embodiment # 1, sample.
Detailed Description
The following table shows 5 specific embodiments of glassy electrode materials of lithium ion batteries according to the present invention:
name of table number
Numbering Li 2 O V 2 O 5 Fe 2 O 3 P 2 O 5 F
1# 10 20 0 70 20
2# 10 10 10 70 20
3# 10 0 20 70 20
4# 10 20 0 70 0
5# 10 30 0 60 20
Example 1#
1) The raw material 30g is accurately weighed according to the composition ratio 1# in table 1, and is put into an agate mortar for grinding and uniformly mixing. The lithium element is introduced together through lithium carbonate and lithium fluoride, the vanadium element is introduced through vanadium pentoxide, the iron element is introduced through ferric oxide, the phosphorus element is introduced through ammonium dihydrogen phosphate, and the fluorine element is introduced through lithium fluoride.
2) And putting the uniformly mixed raw materials into a corundum crucible, putting the corundum crucible into a silicon carbide rod resistance furnace, and melting for 30min at 1250 ℃ to obtain molten and clarified glass liquid.
3) And pouring the obtained molten clear glass liquid on a mold at 250 ℃, transferring the glass to a template at room temperature after the glass is solidified, and naturally cooling.
4) And placing the prepared glass material in an agate mortar, grinding the glass material into fine particles, adding absolute ethyl alcohol, grinding the fine particles by a wet method to obtain 3h glass powder with moderate particle size, and drying the glass powder to obtain the glassy state electrode material of the lithium ion battery.
The sample prepared from the formulation # 1 provided in this example was analyzed by X-ray diffraction and the result is shown in fig. 1 as a glassy material. The obtained glassy state electrode material of the lithium ion battery is prepared into a positive electrode material according to requirements, a battery-grade lithium sheet is used as a negative electrode material, and lithium hexafluorophosphate serving as a main component is used as an electrolyte to assemble a button battery for electrochemical performance test. The voltage range of the cyclic performance test is 0-3V, the current density is 0.05A/g, the initial discharge specific capacity can reach 120 m Ah/g, and the cyclic performance result is shown in figure 2. The charge and discharge curves at a current density of 0.05A/g are shown in FIG. 3.
Example 2#
1) 30g of raw materials are accurately weighed according to the composition ratio of No. 2 in the table 1, put into an agate mortar for grinding and mixed evenly. The lithium element is introduced together through lithium carbonate and lithium fluoride, the vanadium element is introduced through vanadium pentoxide, the iron element is introduced through ferric oxide, the phosphorus element is introduced through ammonium dihydrogen phosphate, and the fluorine element is introduced through lithium fluoride.
2) And putting the uniformly mixed raw materials into a corundum crucible, putting the corundum crucible into a silicon-carbon rod resistance furnace, and melting for 30min at 1250 ℃ to obtain molten and clarified glass liquid.
3) And pouring the obtained molten clear glass liquid on a mold at 250 ℃, transferring the glass to a template at room temperature after the glass is solidified, and naturally cooling.
4) And placing the prepared glass material in an agate mortar, grinding the glass material into fine particles, adding absolute ethyl alcohol, grinding for 3 hours by a wet method to obtain glass powder with moderate particle size, and drying to obtain the glassy state electrode material of the lithium ion battery.
The sample prepared from the formulation # 2 provided in this example was analyzed by X-ray diffraction and tested to be a glassy material. The obtained glassy state electrode material of the lithium ion battery is prepared into a positive electrode material according to requirements, a battery-grade lithium sheet is taken as a negative electrode material, and lithium hexafluorophosphate serving as a main component is taken as electrolyte to assemble the button battery for electrochemical performance test. The voltage range of the cycle performance test is 0-3V, the current density is 0.05A/g, the first discharge specific capacity can reach 100m Ah/g, and the capacity retention rate is 89% after 10 cycles.
Example 3#
1) 30g of raw materials are accurately weighed according to the composition ratio of No. 3 in the table 1, put into an agate mortar for grinding and mixed evenly. The lithium element is introduced together through lithium carbonate and lithium fluoride, the vanadium element is introduced through vanadium pentoxide, the iron element is introduced through ferric oxide, the phosphorus element is introduced through ammonium dihydrogen phosphate, and the fluorine element is introduced through lithium fluoride.
2) Putting the uniformly mixed raw materials into a corundum crucible, putting the corundum crucible into a silicon carbide rod resistance furnace, and melting for 30min at 1250 ℃ to obtain molten and clarified glass liquid
3) And pouring the obtained molten clear glass liquid on a mold at 250 ℃, transferring the glass to a template at room temperature after the glass is solidified, and naturally cooling.
4) And placing the prepared glass material in an agate mortar, grinding the glass material into fine particles, adding absolute ethyl alcohol, grinding for 3 hours by a wet method to obtain glass powder with moderate particle size, and drying to obtain the glassy state electrode material of the lithium ion battery.
The sample prepared from the 3# formulation provided in this example was analyzed by X-ray diffraction and tested to be a glassy material.
Example 4
1) 30g of raw materials are accurately weighed according to the composition ratio of No. 4 in the table 1, put into an agate mortar for grinding and mixed evenly. The lithium element is introduced together through lithium carbonate and lithium fluoride, the vanadium element is introduced through vanadium pentoxide, the iron element is introduced through ferric oxide, the phosphorus element is introduced through ammonium dihydrogen phosphate, and the fluorine element is introduced through lithium fluoride.
2) And putting the uniformly mixed raw materials into a corundum crucible, putting the corundum crucible into a silicon carbide rod resistance furnace, and melting for 30min at 1250 ℃ to obtain molten and clarified glass liquid.
3) And pouring the obtained molten clear glass liquid on a mold at 250 ℃, transferring the glass to a template at room temperature after the glass is solidified, and naturally cooling.
4) And (3) placing the prepared glass material in an agate mortar, grinding the glass material into fine particles, adding absolute ethyl alcohol, grinding for 3 hours by a wet method to obtain glass powder with moderate particle size, and drying to obtain the glassy state electrode material of the lithium ion battery.
The sample prepared from the formulation # 4 provided in this example was analyzed by X-ray diffraction and the test result was a glassy material.
Example 5
1) 30g of raw materials are accurately weighed according to the composition ratio of No. 5 in the table 1, put into an agate mortar for grinding and mixed evenly. The lithium element is introduced together through lithium carbonate and lithium fluoride, the vanadium element is introduced through vanadium pentoxide, the iron element is introduced through ferric oxide, the phosphorus element is introduced through ammonium dihydrogen phosphate, and the fluorine element is introduced through lithium fluoride.
2) And putting the uniformly mixed raw materials into a corundum crucible, putting the corundum crucible into a silicon carbide rod resistance furnace, and melting for 30min at 1250 ℃ to obtain molten and clarified glass liquid.
3) And pouring the obtained molten clear glass liquid on a mold at 250 ℃, transferring the glass to a template at room temperature after the glass is solidified, and naturally cooling.
4) And placing the prepared glass material in an agate mortar, grinding the glass material into fine particles, adding absolute ethyl alcohol, grinding for 3 hours by a wet method to obtain glass powder with moderate particle size, and drying to obtain the glassy state electrode material of the lithium ion battery.
The sample prepared from the formulation # 5 provided in this example was analyzed by X-ray diffraction and the test result was a glassy material.

Claims (11)

1. The glassy state electrode material of the lithium ion battery is characterized by comprising the following raw materials in percentage by weight: 5 to 30 percent of lithium source compound; 0 to 40 percent of vanadium source compound; 0 to 40 percent of iron source compound; 40 to 90 percent of phosphorus source compound; 5 to 30 percent of fluorine source compound.
2. The glassy electrode material of claim 1, wherein the material is glassy, structurally ordered at a short range, disordered at a long range, and free of characteristic peaks in an XRD pattern.
3. The glassy electrode material of claim 1, wherein the lithium source compound is one or more of lithium carbonate, lithium hydroxide, and lithium fluoride.
4. The glassy electrode material of the lithium ion battery of claim 1, wherein the vanadium source compound is one or more of vanadium pentoxide, ammonium metavanadate, vanadium hydroxide, and vanadium tetrafluoride.
5. The glassy electrode material of a lithium ion battery according to claim 1, wherein the iron source compound is one or more of iron oxide, iron hydroxide, iron fluoride.
6. The glassy electrode material of claim 1, wherein the phosphorus source compound is one or more of phosphorus pentoxide, ammonium dihydrogen phosphate, and ammonium monohydrogen phosphate.
7. The glassy electrode material of claim 1, wherein the fluorine source compound is one or more of lithium fluoride, ferric fluoride, hydrofluoric acid, vanadium tetrafluoride, and ammonium fluoride.
8. The method for preparing the glassy electrode material of the lithium ion battery according to claim 1, which comprises the following steps:
(1) Designing the components according to a formula, accurately weighing a lithium source compound, a vanadium source compound, an iron source compound, a phosphorus source compound and a fluorine source compound, and grinding in a mortar to uniformly mix the materials;
(2) Putting the uniformly mixed raw materials into a corundum crucible, putting the corundum crucible into a silicon carbide rod resistance furnace, and melting for 30-60 min at 1200-1300 ℃ to obtain molten and clarified glass liquid;
(3) Pouring the obtained molten clear glass liquid on a preheated mold at 200-250 ℃, transferring the glass liquid to a template at room temperature after the glass is solidified, and naturally cooling the glass liquid;
(4) And (3) mixing 2-4 h by adopting dry grinding or wet grinding to obtain glass powder with moderate granularity, and drying to obtain the glassy state electrode material of the lithium ion battery.
9. A lithium ion battery positive electrode material is characterized by comprising the glassy state electrode material of the lithium ion battery in claim 1 as an active material, and a conductive agent and a binder which are jointly formed into the lithium ion battery positive electrode material.
10. The lithium ion battery positive electrode material of claim 9, wherein the active material mass is 60 wt% to 90 wt% of the lithium ion battery positive electrode material.
11. The lithium ion battery cathode material according to claim 9, wherein the mass of the conductive agent is 10 wt% -30 wt% of the lithium ion battery cathode material.
CN202110375525.3A 2021-04-09 2021-04-09 Novel glassy state electrode material of lithium ion battery and preparation method thereof Pending CN115207295A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2989176B1 (en) * 1998-10-02 1999-12-13 泉陽硝子工業株式会社 Electrically conductive glass composition
CN1875506A (en) * 2003-10-31 2006-12-06 丰田自动车株式会社 Electroactive material and use thereof
CN101689632A (en) * 2007-04-13 2010-03-31 丰田自动车株式会社 Active electrode material, manufacturing method of the same, and lithium-ion battery using such an active electrode material
CN107251283A (en) * 2015-02-25 2017-10-13 国立大学法人长冈技术科学大学 Basic ion active material for anode of secondary cell

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2989176B1 (en) * 1998-10-02 1999-12-13 泉陽硝子工業株式会社 Electrically conductive glass composition
CN1875506A (en) * 2003-10-31 2006-12-06 丰田自动车株式会社 Electroactive material and use thereof
CN101689632A (en) * 2007-04-13 2010-03-31 丰田自动车株式会社 Active electrode material, manufacturing method of the same, and lithium-ion battery using such an active electrode material
CN107251283A (en) * 2015-02-25 2017-10-13 国立大学法人长冈技术科学大学 Basic ion active material for anode of secondary cell

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
TAKUYA AOYAGI等: "Electrochemical Properties and In-situ XAFS Observation of Li2O-V2O5-P2O5-Fe2O3 Quaternary-glass and Crystallized-glass Cathodes", 《JOURNAL OF NON-CRYSTALLINE SOLIDS》, 29 September 2016 (2016-09-29), pages 28 - 35, XP029802880, DOI: 10.1016/j.jnoncrysol.2016.09.016 *

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